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Application of micro-electrospray liquid chromatography techniques to FT-ICR MS to enable high-sensitivity biological analysis

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Journal of the American Society for Mass Spectrometry

Abstract

A microbore electrospray (ESI) injection system has been adapted to our 9.4-tesla ESI FT-ICR mass spectrometer, greatly enhancing the stability and sensitivity of the system. Spray was generated from micro-ESI needles made from sharply tapered, polished fused silica capillaries of 25 to 50 µm inner diameter. Micro-ESI permits low-level sample analysis by constant infusion at sub-µL/min flow rate over a wide range of solvent conditions in both positive- and negative-ion mode. The system is flexible and allows rapid conversion to allow routine LC/MS analysis on low-level mixtures presented in biological media. LC/MS analyses were accomplished by replacing micro-ESI needles with capillaries packed with reverse phase retention media to permit analyte concentration and purification prior to analysis (micro-ESI/LC). A unique nano-flow LC pumping system was developed, capable of producing a true unsplit solvent gradient at flow rates below 1 µL/min. The micro-ESI/LC FT-ICR system produces mass spectra from a mixture of three neuroactive peptides at a concentration of 500 amol/µL (5 fmol each total loaded) in biological salts with baseline separation, signal-to-noise ratio of >10:1 and mass resolving power >5000. These results represent a reduction in detection limit by a factor of ∼2 × 106 over the best previously published LC/FT-ICR MS data.

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Authors and Affiliations

  1. Center for Interdisciplinary Magnetic Resonance, National High Magnetic Field Laboratory, Florida State University, 1800 East Paul Dirac Drive, 32310, Tallahassee, FL

    Mark R. Emmett, Forest M. White (Member), Christopher L. Hendrickson, Stone D. -H. Shi (Member) & Alan G. Marshall (Member)

  2. Department of Chernistry, Florda State University, USA

    Forest M. White (Member), Stone D. -H. Shi (Member) & Alan G. Marshall (Member)

Authors
  1. Mark R. Emmett
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  2. Forest M. White
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  3. Christopher L. Hendrickson
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  4. Stone D. -H. Shi
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  5. Alan G. Marshall
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Correspondence to Alan G. Marshall.

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Emmett, M.R., White, F.M., Hendrickson, C.L. et al. Application of micro-electrospray liquid chromatography techniques to FT-ICR MS to enable high-sensitivity biological analysis. J Am Soc Mass Spectrom 9, 333–340 (1998). https://doi.org/10.1016/S1044-0305(97)00287-0

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  • DOI: https://doi.org/10.1016/S1044-0305(97)00287-0

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